Designation: D 6450 – 99
An American National Standard
Standard Test Method for
Flash Point by Continuously Closed Cup (CCCFP) Tester1
This standard is issued under the fixed designation D 6450; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
2. Referenced Documents
2.1 ASTM Standards:
D 4057 Practice for Manual Sampling for Petroleum and
Petroleum Products2
D 4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products2
E 300 Practice for Sampling Industrial Chemicals3
2.2 ISO Standards:4
ISO Guide 34 Quality Systems Guidelines for the Production of Reference Materials
ISO Guide 35 Certifications of Reference Material – General and Statistical Principles
1. Scope
1.1 This flash point test method is a dynamic method and
depends on definite rates of temperature increase. It is one of
the many flash point test methods available, and every flash
point test method, including this one, is an empirical method.
NOTE 1—Flash point values are not a constant physical-chemical
property of materials tested. They are a function of the apparatus design,
the condition of the apparatus used, and the operational procedure carried
out. Flash point can therefore only be defined in terms of a standard test
method, and no general valid correlation can be guaranteed between
results obtained by different test methods or with test apparatus different
from that specified.
1.2 This test method covers the determination of the flash
point of fuel oils, lube oils, solvents, and other liquids by a
continuously closed cup tester. The measurement is made on a
test specimen of 1 mL.
1.3 This test method utilizes a closed but unsealed cup with
air injected into the test chamber.
1.4 This test method is suitable for testing samples with a
flash point from 10 to 250°C.
3. Terminology
3.1 Definitions:
3.1.1 flash point, n—the lowest temperature corrected to a
pressure of 101.3 kPa at which application of an ignition
source causes the vapors of a specimen of the sample to ignite
momentarily under specified conditions of the test.
3.1.1.1 Discussion—For the purpose of this test method, the
test specimen is deemed to have flashed when the hot flame of
the ignited vapor causes an instantaneous pressure increase of
at least 20 kPa inside the closed measuring chamber.5
3.2 Definitions of Terms Specific to This Standard:
3.2.1 dynamic, adj—the condition in which the vapor above
the test specimen and the test specimen are not in temperature
equilibrium at the time at which the ignition source is applied.
NOTE 2—Flash point determinations below 10°C and above 250°C can
be performed; however, the precision has not been determined below and
above these temperatures.
1.5 If the user’s specification requires a defined flash point
method other than this test method, neither this test method nor
any other method should be substituted for the prescribed
method without obtaining comparative data and an agreement
from the specifier.
1.6 The values stated in SI units are to be regarded as
standard. Temperatures are in degrees Celsius, pressure in
kilo-pascals. The values in parentheses are for information
only.
1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard
statements, see Note 6.
4. Summary of Test Method
4.1 The lid of the test chamber is regulated to a temperature
at least 18°C below the expected flash point. A 1 6 0.1 mL test
specimen of a sample is introduced into the sample cup,
ensuring that both specimen and cup are at a temperature at
least 18°C below the expected flash point, cooling if necessary.
The cup is then raised and pressed onto the lid of specified
dimensions to form the continuously closed but unsealed test
chamber with an overall volume of 4.0 6 0.2 mL.
2
Annual Book of ASTM Standards, Vol 05.02.
Annual Book of ASTM Standards, Vol 15.05.
Available from American National Standards Institute, 11 W 42nd Street, 13th
Floor, New York, NY 10017.
5
The method of detecting the flash point by monitoring the instantaneous
pressure increase is covered by a patent. Interested parties are invited to submit
information regarding the identification of an alternative(s) to this patented item to
ASTM Headquarters. Your comments will receive careful consideration at a meeting
of the responsible technical committee, which you may attend.
3
4
1
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.08 on Volatility.
Current edition approved Aug. 10, 1999. Published October 1999.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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D 6450
but shall not be a tight seal to ensure ambient barometric
pressure inside the test chamber during the test. Critical
dimensions are shown in Fig. A1.2. The pressure inside the
measuring chamber during the temperature increase is monitored. A seal that is too tight results in a pressure increase
above ambient due to the temperature and the vapor pressure of
the sample. A poor heat contact results in a bigger temperature
difference between the sample and the heated lid.
6.1.2 Sample Cup—The sample cup shall be made of
nickel-plated aluminum or other material with similar heat
conductivity. It shall have an overall volume of 4 mL and shall
be capable of containing 1 6 0.1 mL of sample. The critical
dimensions and requirements are shown in Fig. A1.2.
6.1.3 Specimen Temperature Sensor—The specimen temperature sensor (Fig. A1.1: Ts) shall be a thermocouple
(NiCr-Ni or similar) in stainless steel of 1-mm diameter with a
response time of t(90) 5 3 s. It shall be immersed to a depth of
at least 2 mm into the specimen. It shall have a resolution of
0.1°C and a minimum accuracy of 6 0.2°C, preferably with a
digital readout.
6.1.4 Magnetic Stirring—The apparatus shall have provisions for stirring the sample. A rotating magnet outside the
sample cup shall drive a small stirring magnet, which is
inserted into the sample cup after sample introduction. The
stirring magnet shall have a diameter of 3 6 0.2 mm and a
length of 12 6 1 mm. The rotation speed of the driving magnet
shall be between 250 and 270 rev/min.
6.1.5 Air Introduction—The apparatus shall have provisions
for introduction of 1.5 6 0.5 mL of air immediately after each
flash test. The air shall be introduced by a short air pulse from
a small membrane compressor by means of a T-inlet in the
connecting tube to the pressure transducer.
6.1.6 Electrical heating and thermoelectric cooling of the lid
(Fig. A1.1: PE) shall be used to regulate the temperature of the
test chamber for the duration of the test. The temperature
regulation shall have a minimum accuracy of 6 0.2°C.
6.1.7 A high voltage electric arc shall be used for the
ignition of the flammable vapor. The energy of the arc shall be
3 6 0.5 mJ (3 6 0.5 Ws) per arc, and the energy shall be
applied within 43 6 3 ms.
4.2 After closing the test chamber, the temperatures of the
test specimen and the regulated lid are allowed to equilibrate to
within 1°C. Then the lid is heated at a prescribed, constant rate.
For the flash tests, an arc of defined energy is discharged inside
the test chamber at regular intervals. After each ignition, 1.5 6
0.5 mL of air is introduced into the test chamber to provide the
necessary oxygen for the next flash test. The pressure inside the
continuously closed but unsealed test chamber remains at
ambient barometric pressure, except for the short time during
the air introduction and except at a flash point.
4.3 After each arc, the instantaneous pressure increase
above the ambient barometric pressure inside the test chamber
is monitored. When the pressure increase exceeds a defined
threshold, the temperature at that point is recorded as the
uncorrected flash point.
5. Significance and Use
5.1 The flash point temperature is one measure of the
tendency of the test specimen to form a flammable mixture
with air under controlled laboratory conditions. It is only one
of a number of properties that must be considered in assessing
the overall flammability hazard of a material.
5.2 Flash point is used in shipping and safety regulations to
define flammable and combustible materials and classify them.
Consult the particular regulation involved for precise definitions of these classifications.
5.3 This test method can be used to measure and describe
the properties of materials in response to heat and an ignition
source under controlled laboratory conditions and shall not be
used to describe or appraise the fire hazard or fire risk of
materials under actual fire conditions. However, results of this
test method may be used as elements of a fire risk assessment,
which takes into account all of the factors that are pertinent to
an assessment of the fire hazard of a particular end use.
5.4 Flash point can also indicate the possible presence of
highly volatile and flammable materials in a relatively nonvolatile or nonflammable material, such as the contamination
of lubricating oils by small amounts of diesel fuel or gasoline.
6. Apparatus
6.1 Flash Point Apparatus, Continuously Closed Cup
Operation—The type of apparatus suitable for use in this test
method employs a lid of solid brass, the temperature of which
is controlled electrically. Two temperature sensors for the
specimen and the lid temperatures, two electrically insulated
pins for a high voltage arc, and a connecting tube for the
pressure monitoring and the air introduction are incorporated in
the lid. Associated equipment for electrically controlling the
chamber temperature is used, and a digital readout of the
specimen temperature is provided. The apparatus and its
critical elements are shown in Figs. A1.1 and A1.2.6
6.1.1 Test Chamber—The test chamber is formed by the
sample cup and the temperature controlled lid and shall have an
overall volume of 4 6 0.2 mL. A metal to metal contact
between the lid and the sample cup ensures good heat contact
NOTE 3—Caution: Because samples containing low flash material or
having a flash point below the preset initial temperature can oversaturate
the vapor inside the chamber and hence prohibit the detection of a flash
point in the chosen range, the design of the apparatus should incorporate
step-wise ignitions in steps of 10°C, following the closing of the
measuring chamber and before the sample reaches the initial temperature
of the test.
6.1.8 The pressure transducer for the flash point detection
shall be connected to the connecting tube in the lid and shall
have a minimum operational range from 80 to 177 kPa with a
minimum resolution of 0.1 kPa and a minimum accuracy of
60.5 kPa. It shall be capable of detecting an instantaneous
pressure increase above barometric pressure of a minimum of
20 kPa within 100 ms.
NOTE 4—The monitoring of the instantaneous pressure increase above
barometric pressure is one of several methods used to determine a flash
inside the test chamber. A pressure increase of 20 kPa corresponds to a
flame volume of approximately 1.5 mL.
NOTE 5—An automatic barometric correction, which is performed in
6
Continuously closed cup testers meeting these requirements are available from
Grabner Instruments, A-1220 Vienna, Dr. Otto Neurathgasse 1, Austria.
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D 6450
9. Quality Control Checks
9.1 Verify the performance of the instrument at least once
per year by determining the flash point of a certified reference
material (CRM) such as those listed in Appendix X1, which is
reasonably close to the expected temperature range of the
samples to be tested. The material shall be tested in accordance
with Section 11 of this test method, and the observed flash
point obtained in 11.11 shall be corrected for barometric
pressure as described in Section 12. The flash point shall be
within the limits stated in Table X1.1.
9.2 Once the performance of the instrument has been
verified, the flash point of secondary working standards
(SWSs) can be determined along with their control limits.
These secondary materials can then be utilized for more
frequent performance checks. (see Appendix X1). A performance check with a SWS shall be performed every day the
instrument is in use.
9.3 When the flash point obtained is not within the limits
stated in 9.1 or 9.2, follow the manufacturer’s instruction for
cleaning and maintenance and check the instrument calibration
(see Section 10). After any adjustment, repeat the test in 9.1 or
9.2, using a fresh test specimen, with special attention to the
procedural details prescribed in this test method.
accordance with the procedure described in 12.1, can be installed in the
tester. The absolute pressure reading of the pressure transducer described
in 6.1.8 may be used for the correction.
6.1.9 The introduction of a test portion of 1.0 6 0.1 mL
shall be accomplished by the use of a pipette or syringe of the
required accuracy.
7. Reagents and Materials
7.1 Purity of Reagents—Use only chemicals of purity requested in Table X1.1. Unless otherwise indicated, it is
intended that all reagents conform to the specifications of the
Committee on Analytical Reagents of the American Chemical
Society where such specifications are available.7 Other grades
may be used, provided it is first ascertained that the reagent is
of sufficient purity to permit its use without lessening the
accuracy of the determination.
7.1.1 Anisole—Warning—See Note 6.
7.1.2 Dodecane—Warning—See Note 6.
7.2 Cleaning Solvents—Use only noncorrosive solvents capable of cleaning the sample cup and the lid. Two commonly
used solvents are toluene and acetone.
NOTE 6—Warning: Anisole, dodecane, toluene, acetone, and many
solvents are flammable and are health hazards. Dispose of solvents and
waste material in accordance with local regulations.
NOTE 8—Caution: The use of single component verification materials,
such as those listed in Table X1.1, will only prove the calibration of the
equipment. It will not check the accuracy of the entire test method,
including sample handling, because losses due to evaporation will not
affect the flash point as happens with losses of light ends in multicomponent mixtures.
8. Sampling
8.1 Obtain at least a 50 mL sample from a bulk test site in
accordance and instruction given in Practice D 4057, D 4177,
or E 300. Store the sample in a clean, tightly sealed container
at a low temperature.
8.2 Do not store samples for an extended period of time in
gas permeable containers, such as plastic, because volatile
material may diffuse through the walls of the container.
Discard samples in leaky containers and obtain new samples.
8.3 Erroneously high flash points can be obtained when
precautions are not taken to avoid loss of volatile material. Do
not open containers unnecessarily. Do not make a transfer
unless the sample temperature is at least 18°C below the
expected flash point. When possible, perform the flash point as
the first test.
8.4 Samples of very viscous materials may be warmed until
they are reasonably fluid before they are tested. However, do
not heat the unsealed sample above a temperature of 18°C
below its expected flash point.
8.5 Samples containing dissolved or free water may be
dehydrated with calcium chloride or by filtering through a
qualitative filter paper or a loose plug of dry absorbent cotton.
Warming the sample is permitted, but do not heat the sample
above a temperature of 18°C below its expected flash point.
10. Calibration
10.1 Pressure Transducer:
10.1.1 Check the calibration of the pressure transducer
when needed as indicated from the quality control checks
performed in accordance with Section 9. The calibration of the
transducer is checked, using the ambient barometric pressure
as a reference.
10.1.2 If the displayed atmospheric pressure is not equal to
the ambient barometric pressure, adjust the transducer control
until the appropriate reading is observed. The ambient barometric pressure is the actual station pressure at the location of
the tester at the time of measurement.
NOTE 9—Caution: Many aneroid barometers, such as those used at
weather stations and airports, are precorrected to give sea level readings:
These shall not be used for calibration of the apparatus.
10.2 Temperature Sensor—Check the calibration of the
temperature sensor used to monitor the temperature of the
sample when needed as indicated from the quality control
checks (see Section 9). Use only reference thermometers that
are traceable to the National Institute of Standards and Technology (NIST) or national authorities in the country in which
the equipment is used.
NOTE 7—Caution: If the sample is suspected of containing volatile
components, the treatment described in 8.4 and 8.5 should be omitted.
11. Procedure
11.1 Thoroughly clean and dry the lid together with the arc
pins and the sample cup before starting the test, being sure to
remove any solvent used to clean the apparatus. If the expected
flash point of a sample is more than 15°C higher than the flash
point of the previous sample, heat the lid together with an
7
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, D.C. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
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D 6450
result. The initial temperature for this fresh test specimen shall
be 18°C below the temperature of the previous approximate
result.
11.13 Record the specimen temperature reading at the
detected flash point as the uncorrected flash point temperature.
If no flash point was detected within the tested temperature
range, record flash point is higher than the final temperature.
11.14 At the conclusion of the test, cool the sample cup
below 50°C to withdraw it safely.
empty, dry sample cup to a temperature 30°C higher than the
expected flash point of the new sample.
NOTE 10—The dry cup heating procedure will eliminate possible cross
contamination from residual vapors.
11.2 Expected Flash Point—Set the initial temperature to at
least 18°C below the expected flash point. Set the final
temperature to a value beyond the expected flash point.
11.2.1 No Expected Flash Point Available—When testing
materials for which no expected flash point temperature is
known, set the initial temperature to 10°C and measure the
material to be tested in the manner described. This flash point
result shall be considered as approximate. The derived value
can be used as the expected flash point when a fresh specimen
is tested in the standard mode of operation.
11.3 Set the heating rate to 5.5 6 0.5°C/min.
11.4 Set the ignition frequency to 1°C.
11.5 Set the air introduction to 1.5 mL.
11.6 Set the pressure threshold for the flash detection to 20
kPa.
11.7 Initiate the test procedure to regulate the lid to the
initial temperature. When the initial temperature is reached as
indicated by the instrument, prepare to introduce the 1 6 0.1
mL specimen of the sample.
11.8 Ensure that the sealed sample and the sample cup are at
least 18°C below the expected flash point temperature, cool if
necessary. Shake the sample thoroughly before opening the
sample container. Extract 1 mL of sample with a pipette or
syringe, and close the container. Transfer 1 6 0.1 mL of the
sample to be tested into the sample cup.
11.9 Insert a stirring magnet into the sample cup to ensure a
consistent sample mix.
11.10 Put the sample cup onto the sample cup support of the
tester, and start the procedure. Raise and press the sample cup
onto the lid, which is at the initial temperature and thus at a
higher temperature than the sample cup. While the temperature
of the sample cup and the lid are equalizing, apply a precautionary arc at 10°C intervals (see Note 3). If a flash is detected
at one of these precautionary arcs, discontinue the test, and
discard the result. Repeat the test with a fresh specimen and
with a lower initial temperature of at least 18°C below the
temperature at which the flash was detected.
11.11 After the temperature between the temperature regulated lid and the specimen have equalized to within 1°C, start
the actual test for the flash point. Heat the lid with the
programmed heating rate, and apply the arc ignition in equidistant temperature steps of 1°C. Moniter the instantaneous
pressure increase within 100 ms after the arc. Stop the test
when a flash is detected or when the final temperature is
reached in the case of no flash point. The flash point temperature is the specimen temperature at which the instantaneous
pressure increase, due to the presence of the flash, exceeds 20
kPa.
11.12 When a flash is detected at a temperature that is
higher than 26°C above the initial temperature, or when a flash
is detected at a temperature that is less than 10°C above the
initial temperature, consider the result approximate and repeat
the test with a fresh test specimen. Adjust the expected flash
point for this next test to the temperature of the approximate
12. Calculation
12.1 Barometric Pressure Correction—Observe and record
the ambient barometric pressure at the time of the test. When
the pressure differs from 101.3 kPa, correct the flash point as
follows:
Corrected flash point 5 C 1 0.25 ~101.3 – p!
(1)
where:
C 5 observed flash point in °C, and
p 5 ambient barometric pressure in kPa.
Round the corrected value to the nearest 0.5°C.
NOTE 11—Caution: The barometric pressure used in this calculation
must be the absolute ambient pressure for the laboratory at the time of the
test. Many aneroid barometers, such as those used at weather stations and
airports, are corrected to give sea level readings: These shall not be used.
13. Report
13.1 Report the corrected flash point as the Test Method
D 6450, CCCFP of the test specimen.
14. Precision and Bias
14.1 The precision data were developed in a 1996 cooperative test program involving ten laboratories and using three
pure chemicals, one pure hydrocarbon, three fuels, and three
lubricating oils. The precision statements for both repeatability
and reproducibility are for flash points between 10 and 250°C
and do not include the No. 6 fuel oil data.8
NOTE 12—The precision derived in the cooperative test program for
No. 6 fuel oil was significantly worse than for the other samples. It has to
be assumed that the procedure described in Section 11 is not applicable for
this kind of sample.
14.2 Precision—The precision of the procedure for CCCFP,
as determined by the statistical examination of the interlaboratory test results, is as follows:
14.2.1 Repeatability—The difference between successive
results obtained by the same operator with the same apparatus
under constant operating conditions on identical test materials
would, in the long run, in the normal and correct operation of
the test method, exceed the following values in only one case
in twenty.
Repeatability
r 5 1.9°C
14.2.2 Reproducibility—The difference between two single
and independent results obtained by different operators working in different laboratories on identical material would, in the
long run, in the normal and correct operation of the test
8
Supporting data have been filed at ASTM Headquarters. Request RR:D021464.
4
D 6450
method, exceed the following values in only one case in
twenty.
Reproducibility R 5 3.1°C
14.2.3 Bias—Since there is no accepted reference material
suitable for determining the bias for the procedure in this test
method, bias has not been determined.
15. Keywords
15.1 continuously closed cup; flammability; flash point
ANNEX
(Mandatory Information)
A1. APPARATUS SPECIFICATIONS
A1.1 See Fig. A1.1 for CCCFP chamber assembly.
TL
TS
Air
P
Lid temperature sensor
Sample temperature sensor
Air inlet
Pressure transducer
HS
PE
Magnet
STM
A1.2 See Fig. A1.2 for lid/cup chamber assembly.
1 Lid with incorporated temperature sensor and electric heating, made of
brass.
2 Sample cup, made of nickel-plated aluminum.
3 1 mL specimen.
4 Specimen temperature sensor (NiCr-Ni thermocouple).
5 Arc pins, made of stainless steel. Arc gap of defined length.
Heat sink
Peltier element
Rotating magnet
Stirring magnet
FIG. A1.1 CCCFP Chamber Assembly
Designation
A
B
C
D
E
F
G
H
I
a
mm
2.5 6 0.2
14 6 0.3
5.5 6 0.2
15 6 0.5
11.5
20
21
30
50
45°
NOTE 1—Finish of the metal to metal contact surfaces of lid and sample
cup: 30 microns.
FIG. A1.2 Lid/Cup Chamber Assembly
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D 6450
APPENDIX
(Nonmandatory Information)
X1. APPARATUS VERIFICATION FLUIDS
X1.1 Certified Reference Material (CRM)—A stable hydrocarbon or other stable petroleum product with a methodspecific flash point established by a method-specific interlaboratory study following RR:D02-10079 guidelines or ISO
Guides 34 and 35.
X1.1.1 Typical values of the flash point corrected for
barometric pressure for some reference materials and their
typical limits are given in Table X1.1 (see Note X1.1).
Suppliers of CRMs (see Note X1.3) will provide certificates
stating the method-specific flash point for each material of the
current production batch. Calculation of the limits for these
other CRMs can be determined from the reproducibility value
of this test method, reduced by interlaboratory effect and then
multiplied by 0.7 (see Research Report RR:S15-1008).9
methods. Other materials, purities, flash point values, and limits can be
suitable when produced in accordance with the practices of RR:D02-1007
guidelines or ISO Guides 34 and 35. Certificates of performance of such
materials should be consulted before use.
NOTE X1.2—Caution: Handle anisole and dodecane with EXTREME
CARE against contamination. Read the manufacturer’s material safety
data sheet before using.
NOTE X1.3—True CRMs can only be developed once an agreed upon
standard test method exists. As this is the first official version of this test
method, certified CRMs cannot exist. The data shown in Table X1.1
pertain to the batch of anisole (purity, mole % 99.7+) and dodecane
(purity, mole % 99.5+) utilized in the precision study. In the absence of
certified CRMs, anisole and dodecane of equivalent purity may be
regarded as an acceptable substitute as long as this condition exists. Once
CRMs are available, other materials, purities, flash point values, and limits
can be suitable when produced in accordance with the practices of
RR:D02-1007 guidelines or ISO Guides 34 and 35. Certificates of
performance of such materials should be consulted before use, as the flash
point value will vary, depending upon the composition of each CRM
batch.
NOTE X1.1—Purities, flash point values, and limits stated for anisole
and dodecane were developed in an ASTM interlaboratory program to
determine suitability of use for performance fluids in flash point test
9
X1.2 Secondary Working Standard (SWS)—A stable hydrocarbon or other petroleum product whose composition is
known to remain appreciably stable.
X1.2.1 Establish the mean flash point and the statistical
control limits (3s) for the SWS, using standard statistical
techniques (see ASTM MNL 710).
Available from ASTM Headquarters.
TABLE X1.1 CCCFP Typical Flash Point Values and Typical
Limits for CRM
Material
Anisole
Dodecane
Purity (Mole %)
99.7+
99.5+
Flash Point (°C)
43.9
79
Limits (°C)
6 1.5
6 2.1
10
Manual on Presentation of Data Control Chart Analysis, 6th Ed. Available
from ASTM Headquarters.
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6